【作者】 刘志滨；

【导师】 王建华；

【作者基本信息】 西北农林科技大学 ， 临床兽医学， 2006， 硕士

【摘要】 疯草是豆科黄芪属和棘豆属有毒植物的总称,也是世界范围内危害草原畜牧业最严重的一类毒草。在我国,疯草广泛分布于西北、华北和西南的广大草原,危害面积达1100万hm2。苦马豆素是疯草主要毒性成分之一,对动物疯草中毒病的防治有重要意义。疯草中苦马豆素的传统提取方法大多应用索氏提取法或者溶剂冷浸法处理草粉,依次经酸化、碱化萃取和硅胶柱层析等逐步纯化,最后对纯化物进行100℃减压油浴升华。其步骤繁琐,周期长,消耗大量有机溶剂。随着对疯草化学成分以及防除利用等方面研究的深入,需要大量的苦马豆素。现有提取方法效率低,需要改进。本研究首先利用40 KHz的超声波清洗器处理疯草粉,建立批量提取苦马豆素的工艺流程;随后应用20 KHz的超声循环提取机处理疯草粉,并对各个步骤做相应改进,以缩短提取周期、节省试剂,提高疯草中苦马豆素的提取效率。1.称取甘肃棘豆草粉1.5 kg,加水,用40 KHz超声波清洗器处理,水提液浓缩除杂后,用正丁醇萃取,正丁醇萃取液用稀酸水萃取,浓缩后的稀酸水萃取液用氨性氯仿萃取,氨性氯仿萃取液浓缩成浸膏,经石蜡油浴升华得到24 mg白色晶体,初步鉴定为苦马豆素,提取率为16 mg/kg。按此流程分别处理毛瓣棘豆、冰川棘豆、变异黄芪,提取率为15 mg/kg、12 mg/kg、17 mg/kg。2.称取2 kg变异黄芪草粉,加水,用20 KHz超声循环提取机处理,并按上述工艺提取,提取率为14 mg/kg。随后应用20 KHz的超声波循环提取机一次处理20 kg变异黄芪草粉,并按上述流程提取,提取率为12 mg/kg。对升华苦马豆素所得副产物(黄色油状)做GC-MS分析,鉴定出八种化合物。3.绘制苦马豆素气相色谱法标准曲线,并做加标回收试验。依据标准工作曲线测得本试验大规模提取的苦马豆素纯度在77.5%～93.6%范围内。更多还原

【Abstract】 Oxytropis and Astragalus species known as Locoweeds are responsible for Locoism and other problems.Locoweeds are mainly distributed on the vast rangeland,exceeding 11 million hectares,in northwest,north and southwest China. As one of the toxins of locoweed,Swainsonine is important to the research of Locoism. Generally swainsonine is extracted by the soxhlet extraction technology or the extraction in cold solvent,then purified gradually with acid liquid、alkali liquid and silica gel column chromatogram etc.Finally the residue was sublimed in 100℃olefin.This technics is unefficient and wastes a lot of solvent.Along with the further research of locoweed,more swainsonine is needed. The former technics was to be advanced.This experiment utilized 40 KHz supersonic cleaner to dispose some locoweed powder firstly , established the flow. Subsequently 20 KHz supersonic circulated extracting machine was utilized to dispose locoweed.The following extracting process was also simplified to shorten the cycle、save the solvent,so as to promote the swainsonine extracting efficiency from locoweed.1. Disposed 1.5 kg O.kansuensis powder with 40KHz ultrasound in water to substitute the traditional soxhlet extraction technology or the extraction in cold solvent,concentrated and removed the impurity,then extracted with n-butanol,which was extracted by sparse acid.Extracted the concentrated acid liquid with ammoniated chloroform.Concentrated the ammoniated chloroform to residue.The residue was sublimed in 100℃olefin and 24 mg white crystal was collected.The crystal was preliminary determined as swainsonine. The extraction rate was 16 mg/kg.Swainsonine was extracted by this technics from O.sericopetala、O.glacialis and A.variabilis,the extracting rate is 15 mg/kg、12 mg/kg and 17 mg/kg.2. Disposed 2 kg A.variabilis powder with 20 KHz ultrasound in water according to the new technics,the extracting rate was 14 mg/kg.Sequently disposed 20 kg A.variabilis powder with 20 KHz ultrasound in water according to the new technics,the extracting rate was 12 mg/kg.The outgrow of subliming swainsonine has been studied by means of the GC-MS,8 compounds was identified.3. Criteria curve of swainsonine liquid and GC peak area was drawn and tested更多还原